Aqueous tape casting and crystallization behavior of gadolinium-doped ceria

An aqueous tape casting of gadolinia-doped ceria (GDC) ceramics was developed using Poly(acrylic acid) PAA as dispersant, Poly(vinyl alcohol) PVA as binder, Poly(ethylene glycol) PEG as plasticizer, and deionized water as solvent. Surface properties of GDC powder with and without PAA dispersant were characterized by electrokinetic measurements. The zeta potential measurement revealed that the isoelectric point for GDC powders in the absence of dispersant corresponds to a pH value of 4.06. The experimental results showed that pH value greatly affects the rheology of the slurry. Homogeneous, smooth, and defect-free green tapes were successfully obtained by using an appropriate slurry formula. Moreover, the crystallization kinetics of GDC powders prepared by coprecipitation process also has been investigated in this study. The activation energy of crystallization was calculated by differential scanning calorimetry (DSC) at different heating rates. Analysis of non-isothermal DSC data presented values of 105.3 kJ/mol and 1.171 for the activation energy of crystallization presented and the Avrami exponent, respectively.     

Aqueous processing of Ce0.8Sm0.2O1.9 green tapes

An aqueous tape casting of Ce_0.8Sm_0.2O_1.9 (SDC) ceramics was developed using poly(acrylic acid) (PAA) as dispersant, poly(vinyl alcohol) (PVA) as binder, poly(ethylene glycol) (PEG) as plasticizer, and deionized water as solvent. Surface properties of SDC powder with and without PAA dispersant were characterized by electrokinetic measurements. The rheology of the SDC slurries was evaluated with a rotary viscometer. The zeta potential measurement showed that the isoelectric point (IEP) for SDC powders in the absence of dispersant corresponds to a pH value of 3.66. The experimental results showed that the pH value greatly affects the rheology of the slurry. The optimum content to get a stable dispersed slurry is 2 wt% PAA in pH value range of 9–10. In presence of 2 wt% PAA dispersant, 55 wt% SDC powders exhibited shear thinning behavior, indicating that SDC slurry was homogenous and well stabilized. Homogeneous, smooth, and defect-free green tapes were successfully obtained by an appropriate slurry formula.     

Study on enhancement of diamond nucleation on fused silica substrate by ultrasonic pretreatment

Fused silica substrates were pretreated by the ultrasonic vibration in the diamond powder slurry (UVDS). The influence of UVDS parameters such as the grain size of diamond powder, the liquid medium used to form the slurry, the weight ratio of diamond powder to liquid medium and the pretreatment time on the diamond nucleation density (DND) were systemically investigated. The grain size of diamond powder greatly affected the DND, the larger the grain size the higher the DND in our experiment conditions. The DND was about the same using acetone or ethanol or hexane medium. The best weight ratio of diamond powder (grain size 20–40 μm) to liquid medium was ∼1/60. Under appropriate pretreatment and CVD conditions, the DND of ∼10¹⁰ cm⁻² was obtained on fused silica substrates. Continuous ultra-thin diamond films with uniform and smooth surface (diamond grain size: ∼150 nm and surface roughness: ∼6 nm) were synthesized in an improved hot filament chemical vapor deposition (HFCVD) system. Nano-damaged sites on the pretreated surface mainly enhanced the DND and shortened the incubation time of nucleation.     

Stabilization of alumina with polyelectrolyte and comb copolymer in solvent mixtures of water and alcohols

Solvent mixtures of water and ethanol and water and isopropanol have been evaluated for processing of concentrated alumina suspensions. The addition of alcohols may increase the long-term stability of suspensions with soluble ceramic species such as magnesia, which is added as a sintering aid. A poly(acrylic acid) and a hydrophilic comb copolymer were used as dispersants for the different solvent mixtures. The aim was to compare the stabilization efficiency at normal processing conditions, pH 9–10, through rheological measurements and to develop a robust system including magnesia with long-term stability. The electrostatic stabilization of the dispersants in the different solvent mixtures was studied by zeta potential measurements. Highly negative zeta potentials were observed for the poly(acrylic acid) at pH 9–10 in the solvent mixtures. A charge contribution was also seen from the adsorbed comb copolymer, however smaller than for the poly(acrylic acid). Low viscosity was obtained for suspensions stabilized with poly(acrylic acid) in solvent mixtures with either 25 vol% ethanol or isopropanol. Higher alcohol to water ratio led to flocculation of the suspension when poly(acrylic acid) was used as dispersant. Alumina suspensions with added magnesia in isopropanol:water 25:75 and poly(acrylic acid) as dispersant showed long-term stability. The viscosity remained almost constant during 4 days of aging. Suspensions stabilized with the comb copolymer dispersant gave stable systems with ethanol and isopropanol concentrations between 25 and 75 vol%. The superior dispersing efficiency of the comb copolymer at alcohol contents above 25 vol% was believed to originate from steric stabilization in combination with low effective particle size, giving low viscosity through lower apparent solid contents of the suspension.     

Effect of Solvent on Titania Particle Formation and Morphology in Thermal Hydrolysis of TiCl4

Titania powders were synthesized by the thermal hydrolysis of titanium tetrachloride with the yield of above 85% in a mixed solvent of n -propanol and water. The morphology of the precipitates was controlled by adjusting the volume ratio of n -propanol to water (RH ratio) of the mixed solvent. Precipitates obtained with an RH ratio of 0 were fine, and highly agglomerated. In contrast, an RH ratio of 3 resulted in precipitates consisting of uniform and discrete particles. According to observations of the zeta potentials of precipitates and the dielectric constants of solvents, the discrete particles obtained with an RH ratio of 3 resulted from the low zeta potential and dielectric constant. The result of Fourier transform infrared (FTIR) spectroscopy showed the chemical interaction of particle surface with the solvent alcohol, which decreased the zeta potential of precipitates with an increase of RH ratio. Adding hydroxypropyl cellulose (HPC) as a steric dispersant made it possible to reduce the size of particles to the submicrometer range. Effects of the solvent on the formation and morphology of the resulting particles were investigated.     

乙酸异丙酯-异丙醇-DMSO的等压汽液相平衡和萃取精馏模拟

在101.3 kPa压力下,采用汽液平衡釜测定了二元物系异丙醇+二甲基亚砜（DMSO）、乙酸异丙酯+DMSO和三元物系异丙醇+乙酸异丙酯+DMSO的汽液平衡数据。利用Van Ness点校验法检验以上气液平衡数据,结果表明,数据符合热力学一致性。采用NRTL、Wilson和UNIQUAC活度系数模型对二元数据进行了拟合,并进行了三元物系汽液相平衡数据预测,结果表明,回归数据和实验数据吻合良好。Wilson模型的预测结果优于NRTL和UNIQUAC模型。一定量DMSO的加入可消除异丙醇和乙酸异丙酯的共沸点,因此,DMSO可作为一种有效的萃取剂来萃取精馏分离此二元物系。然后,通过流程模拟软件Aspen Plus,使用获得的二元交互作用参数对三元系统的萃取精馏进行了模拟。讨论了在不同的操作条件（塔板数、进料位置、溶剂比和回流比）下,异丙醇和乙酸异丙酯分离的情况,得到了最适宜的操作条件。     

Relationship between surface μ‐roughness and interface slurry particle spatial distribution during glass polishing

During optical glass polishing, a number of interactions between the workpiece (i.e., glass), polishing slurry, and pad can influence the resulting workpiece roughness at different spatial scale lengths. In our previous studies, the particle size distribution of the slurry, the pad topography, and the amount of material removed by a single particle on the workpiece were shown to strongly correlate with roughness at AFM scale lengths (nm‐μm) and weakly at μ‐roughness scale lengths (μm‐mm). In this study, the polishing slurry pH and the generation of glass removal products are shown to influence the slurry particle spatial and height distribution at the polishing interface and the resulting μ‐roughness of the glass workpiece. A series of fused silica and phosphate glass samples were polished with various ceria and colloidal silica slurries over a range of slurry pH, and the resulting AFM roughness and μ‐roughness were measured. The AFM roughness was largely invariant with pH, suggesting that the removal function of a single particle is unchanged with pH. However, the μ‐roughness changed significantly, increasing linearly with pH for phosphate glass and having a maximum at an intermediate pH for fused silica. In addition, the spatial and height distribution of slurry particles on the pad (as measured by laser confocal microscopy) was determined to be distinctly different at low and high pH during phosphate glass polishing. Also, the zeta potential as a function of pH was measured for the workpiece, slurry, and pad with and without surrogate glass products (K₃PO₄ for phosphate glass and Si(OH)₄ for silica) to assess the role of interfacial charge during polishing. The addition of K₃PO₄ significantly raised the zeta potential, whereas addition of Si(OH)₄ had little effect on the zeta potential. An electrostatic DLVO three‐body force model, using the measured zeta potentials, was used to calculate the particle–particle, particle–workpiece, and particle–pad attractive and repulsive forces as a function of pH and the incorporation of glass products at the interface. The model predicted an increase in particle–pad attraction with an increase in pH and phosphate glass products consistent with the measured slurry distribution on the pads during phosphate glass polishing. Finally, a slurry “island” distribution gap (IDG) model has been formulated which utilizes the measured interface slurry distributions and a load balance to determine the interface gap, the contact area fraction, and the load on each slurry “island”. The IDG model was then used to simulate the workpiece surface topography and μ‐roughness; the results show an increase in roughness with pH similar to that observed experimentally.     

Preparation of transparent poly(vinyl alcohol) hydrogel

A transparent hydrated gel is prepared from a poly(vinyl alcohol)(PVA) solution in a mixed solvent consisting of water and dimethyl sulfoxide(DMSO). Upon cooling the PVA solution below the room temperature, a gel is formed as a consequence of crystallization of PVA molecules. Exchange of DMSO in the formed gel with water gives the hydrated PVA gel which is high in tensile strength, water content, and light transmittance.     

Dual‐bonding structured ternary composite film of poly(vinyl alcohol)–boric acid–nanodiamond

Ternary composite films of poly(vinyl alcohol) (PVA), boric acid (BA), and detonation nanodiamond (DND) were prepared by aqueous solution method. Because of its excellent mechanical/thermal properties and low friction coefficient, DND is expected to offer PVA film superior performance if the puzzles of particle agglomeration in polymer matrix and fragile interface reaction between DND and PVA can be settled. BA was used as a crosslinking agent to form a strong network structure between DND and PVA. Investigation on microstructure of PVA/BA/DND films and bonding mechanisms therein shows that BA, DND, and PVA may crosslink by oxo‐bridges owing to the interaction of hydroxyl groups. The Young's modulus (E) of composite films was enhanced by nearly 3.3 times with only 0.8 wt % DND loading, and the antiwear, thermal stability, and waterproof properties can be significantly improved after the crosslinking. Meanwhile, the transparency of composite films can be well preserved even with large DND content. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45449.     

环境友好型脱漆剂的制备

以苯甲醇(BA)、二丙二醇丁醚(DPNB)和二甲基亚砜(DMSO)等为主溶剂制备环境友好型脱漆剂,采用单因素试验法研究了有机溶剂、促进剂、缓蚀剂以及封闭剂等助剂对脱漆效率的影响。试验结果表明:以BA、DPNB和DMSO为主溶剂,异丙醇(IPA)为助溶剂,表面活性剂AR-10和十二烷基苯磺酸钠(LAS)复配,复配有机酸为促进剂,微晶蜡为封闭剂,氨基磺酸与有机羧酸醇铵盐类缓蚀剂复配。当复合主溶剂的用量范围为60%～70%,m(DMSO)∶m(DPNB)=8∶6,m(AR-10)∶m(LAS)=1∶0.8,复配用量为2.5%～3%,异丙醇用量为5%～l0%,复配有机酸用量为7.5%～10%,微晶蜡用量为2.5%～3%时,脱漆效率最高。其组成均为低挥发性的物质,符合绿色化学"高效、洁净、经济、环保"的要求。     

Effects of solvent adsorption on solution properties of poly(vinyl alcohol)/dimethylsulfoxide/water ternary systems

In this study, the solvent adsorption phenomena of poly(vinyl alcohol) (PVA) in cosolvent mixtures of dimethylsulfoxide (DMSO; solvent 1) and water (solvent 2) were investigated. Typically, this cosolvent mixture could form hydrogen‐bonded DMSO/(water)₂ complexes, involving one DMSO and two water molecules. Because of the complex formation in the cosolvent mixtures, PVA chains preferentially adsorb water molecules at DMSO mole fraction X₁ < 0.33, but preferentially adsorb DMSO molecules at X₁ > 0.33. The preferential adsorption of DMSO (a good solvent for PVA) could cause the relatively extended conformation of PVA chains in solutions because of the increase in excluded volume effect. Because of various interactions between PVA chains and cosolvent mixtures, the aggregation and gelation behaviors of PVA solutions were significantly affected by the composition of cosolvent mixture. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 3211–3217, 2004     

Nonaqueous Spray-Drying as a Route to Ultrafine Ceramic Powders

Spray-drying imparts unique powder handling features to a wide variety of dried products and is usually carried out in a heated airstream while feeding an aqueous suspension of some solid material. The present work, however, explores nonaqueous spray-drying as a means of preparing fine powders of metal oxides. In this case an alcohol solvent was used in place of water and the slurry sprayed under an inert atmosphere. Using the nonaqueous technique, the product consists of distinct but loosely aggregated primary particles.     

A study of solvent exchange process in (ethylene–vinyl alcohol) copolymer gels by a proton nuclear magnetic resonance spectroscopy imaging method

The proton nuclear magnetic resonance (¹H NMR) image patterns of (ethylene–vinyl alcohol) copolymer (EVOH)/dimethylsulfoxide (DMSO) gels with various ethylene contents were measured to elucidate the process of solvent exchange between DMSO and water in the gels soaked in water. The results of these experiments indicate that the rate of solvent exchange between DMSO and water in the gels increased with an increase in the ethylene content of EVOH copolymers. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 504–508, 2002     

阴离子型添加剂对水煤浆动电势的影响

选用了变质程度不同的8种煤和三类共9种分子结构不同的阴离子型添加剂,详细考察了添加剂的结构特征对水煤浆动电势的影响规律．研究结果表明,对于线性高分子型阴离子添加剂聚对苯乙烯磺酸钠（PSS）,在所考察的相对分子量的范围内（5．34万～33．39万）,各煤种的动电势随着分子量的增加而增加（绝对值）．对于萘磺酸甲醛缩合物钠盐添加剂（NSF）,在萘环上引入甲基和苄基取代基时,动电势均有不同程度的降低．对于木质素和腐植酸盐类添加剂,高磺化度也将导致煤粒动电势的降低．     

Relationship between the process parameters and the saturation point in electrophoretic deposition

We used the electrophoretic deposition (EPD) process to fabricate a composite with glass frit and investigated the EPD parameters to find the optimum deposition time by understanding the relationship between the process parameters of zeta potential (ZP), pH, deposition yield and saturation point in a slurry. A binder and a dispersing agent were mixed properly with glass frit (0.2–25 μm, d₅₀ = 8.77 μm) in an ethyl alcohol medium for the preparation of the slurry. The pH and ZP were in an inverse relationship to each other due to the generation of H₃O⁺ ions with the addition of the dispersing agent in the slurry. The acidic nature of the slurry resulted in a decrease of the pH and an increase of the ZP. Otherwise, the pH increased with the addition of the glass frit in the slurry because H₃O⁺ ions were absorbed on the glass frit. Therefore, the OH^? ions correspondingly increased. The saturation point of EPD was strongly correlated with the variation of the pH in the slurry; this is caused by a chemical reaction between the ethyl alcohol and the ions that make up the glass frit. An adjustment of the pH variation and the saturation point in the slurry can be established with respect to the optimum deposition time in the slurry.     

Dispersion of aluminum‐doped zinc oxide nanopowder in non‐aqueous suspensions

This study proposes appropriate dispersants for dispersing aluminum‐doped zinc oxide (AZO) nanopowder in the commonly used organic solvent‐dimethylacetamide (DMAC). The dispersion efficiencies and stabilization mechanisms of four DMAC‐soluble dispersants, poly(acrylic acid) (PAA), polyethyleneimine (PEI), poly(vinyl alcohol) (PVA), and poly(vinyl pyrrolidone) (PVP), are compared. The non‐polyelectrolyte‐based PVA and PVP surprisingly exhibit greater efficiency than the polyelectrolyte‐based PAA and PEI. This is because the nano AZO is soft‐agglomerated in DMAC and easily de‐agglomerated by the application of ultrasonic power; therefore, the increased viscosity contributed from additions of PVA and PVP efficiently prevent reagglomeration and sedimentation of the nanopowder. This stabilization mechanism is evidenced by an experimental analysis of zeta potentials and rheology and also by theoretical calculations based on Stokes’ law.     

分散剂用量对钛酸锶钡水基浆料稳定性的影响

使用聚甲基丙烯酸铵(ammonium polymethacrylate,PMAA-NH4)作为分散剂,研究了不同pH值条件下分散剂用量对钛酸锶钡(Ba0.6Sr0.4TiO3)水基浆料稳定性的影响,并分析了其影响机理.结果表明:PMAA-NH4的加入能够显著提高Ba0.6Sr0.4TiO3粉体的zeta电位,在加入量(质量分数,下同)为0.4%时,zeta电位为负值,达到最小,从而提高了Ba0.6Sr0.4TiO3水基浆料稳定性.在pH值小于8时,会发生Ba0.6Sr0.4TiO3料浆中的Ba2 和Sr2 离子溶出;pH值大于8时,Ba0.6Sr0.4TiO3粉体的zeta电位随PMAA-NH4的加入量的增加而增大.在pH值为8～9,PMAA-NH4的加入量为0.4%时,实现Ba0.6Sr0.4TiO3粉体对PMAA-NH4的饱和吸附,此时浆料的稳定性最好.     

l-Ascorbic acid as a new activator in fabrication of ceramics by techniques using in situ polymerization

The paper reports the development of a new system applicable in shaping techniques using in situ polymerization. The system is based on saccharides derivatives and allows to eliminate harmful processing agents from ceramic slurry. Instead of commonly applied 2-hydroxyethyl acrylate or acrylamide (monomers) and N,N,N′,N′-tetramethylethylenediamine (activator) the compounds based on glucose were used. As a monomer 3-O-acryloyl-d-glucose was applied. As a new activator l-ascorbic acid (also known as vitamin C) was used. Research was carried out for YSZ. As initiators ammonium persulfate and hydrogen peroxide were used. The new system was studied in terms of zeta potential, pH and rheological measurements. Ceramic samples were prepared by gelcasting and gel-tape casting methods. The experiments showed that l-ascorbic acid used as the activator has positive influence on rheological properties of suspensions with YSZ and together with ammonium persulfate allows to form defect free ceramic bodies with a homogenous composition.     

Thermosensitive folic acid-targeted poly (ethylene-<Emphasis Type="Italic">co</Emphasis>-vinyl alcohol) hemisuccinate polymeric nanoparticles for delivery of epirubicin to breast cancer cells

A novel thermosensitive folic acid (FA)-targeted succinylated poly (ethylene-co-vinyl alcohol) (EVOH) (EVOHS-FA) nanocarrier was synthesized for the specific delivery of epirubicin (EPI) to MCF-7 breast cancer cell line. Three different ratios of synthesized EVOH-Suc were reacted with FA. The structure of the desired products (EVOHS₄₀-FA, EVOHS₆₀-FA and EVOHS₈₀-FA) was confirmed by ¹H NMR and FTIR techniques. Nanoparticles were obtained by nano-precipitation procedure using DMSO/H₂O as solvent/anti-solvent. The particle size, zeta potential, entrapment efficacy and in vitro release profile of the final formulations in different temperatures were measured. The optimized nanoparticles had the particle size of 214 ± 8.5 nm, zeta potential of ?29.6 mV, PDI of 0.198 ± 0.04, and a high encapsulation efficiency that released the drug efficiently within 450 h at the temperature of 40 °C compared to 37 °C. The morphology of nanoparticles was studied by scanning electron microscopy. The in vitro cytotoxicity was evaluated using the MTT assay on MCF-7 cell lines in response to temperatures of 37 and 40 °C. The MTT assay indicated that the targeted nanoparticles carrying EPI were significantly more cytotoxic than the non-targeted nanoparticles and the free drug at 40 °C.     

Lipoxygenase-oxidized soap stock as source of hydroxy conjugated octadecadienoic acids

A laboratory procedure was developed for the production of hydroxy conjugated octadecadienoic acids (HOCD). Lipoxygenase oxidation of distilled or crude soap stock produces hydroperoxy conjugated octadecadienoic acids, which can be reduced to HOCD. Crude aqueous soy flour extracts and defatted soy flour are convenient, effective and inexpensive lipoxygenase sources. This new procedure allows high substrate concentrations of 100 mg/ml to be used while achieving 75% to 90% oxidation of the available linoleic acid during a reaction time of 20 to 40 min. Aqueous ethanol and dimethyl sulfoxide (DMSO) solvent systems were compared. The DMSO system produced higher yields of hydroperoxy acids with low enzyme concentrations. Hydroperoxide yields are good when short reaction times, high pH levels and free radical scavengers are used. Presented at the AOCS Meeting, Chicago, September 1970. No. Utiliz. Res. Dev. Div., ARS, USDA.